関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 7a-nitromethyl-2,3,5,6,7,7a-hexahydro-1H-pyrrolizine | HCID 10487359 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (Hexahydro-1H-pyrrolizin-7A-YL)methanamine | HCID 10654304 | 91% |
反応手順
To 5.0 ml of 80% ethanol, 7a-nitromethyl-2,3,5,6,7,7a-hexahydro-1H-pyrrolizine (300 mg, 1.76 mmol, obtained in Example 1) and concentrated hydrochloric acid (0.45 ml, 5.28 mmol) were added to stir for 10 minutes at 20° C. Then, iron powder (500 mg, 8.95 mmol) was added to the mixture to further stirr for 1 hour at 20° C. Insoluble matters were filtered off and the filtrate was concentrated, adding 0.5N NaOH (10 ml) to the residue, filtering the solution to further remove insoluble matters, extracting the filtrate with chloroform, drying the extract over anhydrous sodium sulfate, concentrating the extract, and distilling the resulting crude product to afford 224 mg of the desired compound (Yield: 91%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04985569 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-ff773b7940854008bb0342b5d6a70f3b |
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| 出典メモ | uspto-grants-1991_01 |
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